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建立并验证了一种改良的 QuEChERS 方法,结合超高效液相色谱-串联质谱(UHPLC-MS/MS)技术,用于从啤酒中提取、鉴定和定量多真菌毒素。

Development and validation of an analytical method for the extraction, identification, and quantification of multi-mycotoxins in beer using a modified QuEChERS procedure and UHPLC-MS/MS.

机构信息

Departamento De Química, Centro Federal De Educação Tecnológica De Minas Gerais , Belo Horizonte, Minas Gerais, Brazil.

Instituto Mineiro De Agropecuária , Belo Horizonte, Minas Gerais, Brazil.

出版信息

Food Addit Contam Part A Chem Anal Control Expo Risk Assess. 2020 Dec;37(12):2135-2148. doi: 10.1080/19440049.2020.1812735. Epub 2020 Nov 2.

Abstract

Although beer is one of the most popular alcoholic beverages in the world, there is no specific legislation regarding contaminants, especially mycotoxins, for this product. The present manuscript reports the development and validation of an analytical methodology based on the QuEChERS approach, followed by quantification via UHPLC-MS/MS for the simultaneous determination of seventeen mycotoxins in beer. During the validation, amatrix effect was observed for 82% of the analytes. Linearity and recovery were evaluated using spiked blank samples, and the chosen methodology proved to be efficient for all analytes, with recoveries ranging from 71 to 118%, excepting ergonovine, for which recovery of 57% was achieved. Precision was estimated in terms of repeatability and reproducibility, with variations from 2.6 to 28.2% and 9.7 to 28.7%, respectively. The detection (LOD) and quantification (LOQ) limits, determined from the values of CCα and CCβ, ranged from 0.26 to 117 µgkg and from 0.30 to 135 µgkg, respectively. Measurement uncertainties were based on the bottom-up methodology, with uncertainties ranging from 0.03 to 17 µgkg. Finally, thirty-eight beer samples, collected at the local market, were analysed, and 16 of them showed contamination by deoxynivalenol in concentrations ranging from 159 ± 26 µgkg to 648 ± 106 µgkg.

摘要

尽管啤酒是世界上最受欢迎的酒精饮料之一,但针对该产品,并没有针对污染物(尤其是真菌毒素)的具体法规。本文报告了一种基于 QuEChERS 方法的分析方法的开发和验证,随后通过 UHPLC-MS/MS 进行定量,以同时测定啤酒中的十七种真菌毒素。在验证过程中,观察到 82%的分析物存在基质效应。通过加标空白样品评估了线性和回收率,所选择的方法对所有分析物均有效,回收率范围为 71%至 118%,除了麦角新碱,其回收率为 57%。精密度通过重复性和再现性来评估,变异系数分别为 2.6%至 28.2%和 9.7%至 28.7%。检测限(LOD)和定量限(LOQ),根据 CCα 和 CCβ 值确定,范围分别为 0.26 至 117µgkg 和 0.30 至 135µgkg。测量不确定度基于自上而下的方法,不确定度范围为 0.03 至 17µgkg。最后,分析了在当地市场收集的 38 个啤酒样本,其中 16 个样本被检出脱氧雪腐镰刀菌烯醇污染,浓度范围为 159±26µgkg 至 648±106µgkg。

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